Sodium Hydroxide → HCID 10666287、化合物

HRID 2237338

反応式

HRID 2237338 の反応式
[ClH:1].[NH2:2][CH2:3][CH2:4][S:5][S:6][CH2:7][CH2:8][NH2:9].[OH-:10].[Na+].[Cl:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17]>C1COCC1>[S:5]([CH2:4][CH2:3][NH:2][C:13](=[O:10])[CH2:14][CH2:15][CH2:16][Cl:1])[S:6][CH2:7][CH2:8][NH:9][C:16](=[O:17])[CH2:15][CH2:14][CH2:13][Cl:12]

参加物

5

反応物 3

HCID 14798Sodium Hydroxide2 回HCID 783704-Chlorobutyryl chlorideHCID 1676282-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride

生成物 1

HCID 10666287HCID 10666287、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

60 g of cystamine hydrochloride was solubilized in 500 mL and cooled to 5° C. The pH was raised to 10 by addition of aq. NaOH (30%). A solution of 4-chlorobutanoyl chloride (105 g) in anhydrous THF (500 mL), was added dropwise, while the pH was maintained above 7 by addition of aq. NaOH (30%). After completion of the addition and stabilization of pH at 7, the mixture mixed for 3 days. The aqueous layer was extracted with 3×500 mL dichloromethane, combined with THF layer and dried over Na2SO4. After drying under vacuum, 41 g of a white powder were collected. Analyses were in accordance with the expected structure.

後処理

  1. additionAfter completion of the addition and stabilization of pH at 7
  2. additionthe mixture mixed for 3 days
  3. extractionThe aqueous layer was extracted with 3×500 mL dichloromethane
  4. dry with materialdried over Na2SO4
  5. dry with materialAfter drying under vacuum, 41 g of a white powder
  6. customwere collected

出典と根拠

ORDレコード
ord-0c79e47db59f4b84a45a00062d668bae
出典データセット
uspto-grants-2010_05
特許番号
US07717964B2

関連ノート

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